目的 对高效液相色谱-串联质谱法（HPLC-MS/MS）测定枳壳中禁用农药杀虫脒残留量进行不确定度评估。方法 采用HPLC-MS/MS法对枳壳中杀虫脒残留量进行测定，通过建立数学模型，分析测定过程的主要不确定度来源，对各个分量进行评估。结果 不确定性的主要来源是标准溶液的配制、工作曲线的拟合、重复性及加样回收率引入。当杀虫脒的残留量为0.016 mg/kg时，扩展不确定度为0.002 9 mg/kg（k＝2）。结论 枳壳中禁用农药杀虫脒残留量测定结果准确且重现性好，可用于枳壳中禁用农药多残留的质量控制；建立的不确定度评定法适用于测定中药材及饮片中禁用农药残留量的不确定度分析。

Objective To evaluate the uncertainty of prohibited pesticide chlordimeform residue in Zhiqiao (Aurantii Fructus) determination by high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS). Methods The residue of chlordimeform in Aurantii Fructuswas determined by HPLC-MS/MS. Through the establishment of mathematical model, the main sources of uncertainty in the measurement process were analyzed, and each component was evaluated. Results The main sources of uncertainty were the preparation of standard solution, the fitting of working curve, reproducibility and the recoveries of standard addition. When the residue of chlordimeform was 0.016 mg/kg, the expanded uncertainty was 0.002 9 mg/kg (k= 2). Conclusion This method is suitable for the uncertainty analysis of chlordimeform residue by gas chromatography tandem mass spectrometry, and can provide scientific and reliable basis for the accuracy of pesticide residue measurement results.

R286.2